This research is devoted to the preparation of cerium-containing layered double hydroxides (LDHs) and exploring the possibility of stabilizing cerium in the unstable valence state (III) in their structure. It has been shown that the best result is achieved in the case of using hydrothermal treatment in the synthesis process. A sample of an LDH obtained via this method possesses characteristics typical for this class of compounds, as has been demonstrated using a set of instrumental methods (XRD, IR, TG-DSC). It has been proved by cerium L-3-edge X-ray absorption spectroscopy that cerium is only partially oxidized to Ce(IV) during the synthesis process.